Traditional aluminum halohydrate and aluminum-zirconium-glycine halohydrate salts are soluble only in aqueous solutions. The only alcohol soluble materials that have been prepared so far are aluminum halohydrate compounds that contain very high excess of chloride (Al:Cl.about.1.3), and a controlled moisture content. The high acid condition make these compounds more irritating than the regular antiperspirant products (which have an Al:Cl.about.2), and the high moisture content calls for very specific spray drying conditions that make the manufacturing of these products a rather delicate matter.
Alcohol or other non-aqueous solutions of aluminum-zirconium-glycine halohydrates salts are not well known in the art. This is because glycine is typically not soluble in the non-aqueous medium and methods for producing solid aluminum-zirconium halohydrates (without glycine) is not known in the art.
U.S. Pat. No. 3,359,169 to Slater et al., teaches a method for reacting aluminum and aluminum chlorohydroxides with hydroxylic organic compounds. The aluminum and aluminum chlorohydroxides are produced by contacting an aluminum compound with a hydroxylic reagent in the presence of sufficient water to dissolve the aluminum compound and then removing water from the system by evaporation. The compound prepared by the method taught by Slater et al. have a high degree of solubility in ethyl alcohol and glycols.
U.S. Pat. No. 3,405,153 to Jones et al., teaches a method of making novel metal-aluminum inorganic-organic complexes which are significantly soluble in non-aqueous media. The method comprises (A) mixing an aqueous solution of an aluminum-containing material with a zinc halide or zirconyl halide; (B) adding to that mixture a polyhydroxy compound having at least 2 carbon atoms, each of which is linked to a hydroxy group; (C) heating the mixture to a temperature of from about 50.degree. C. to about 120.degree. C. to evaporate moisture to about 0.8 of original volume; and (D) drying the heated mixture until a constant weight is achieved and the product has a moisture content of from about 0.5 to about 20%. The resulting salts are soluble in non-aqueous solvents, for example ethanol, in concentrations of at least 10%.
U.S. Pat. No. 3,420,932 to Jones et al., teaches a method of making inorganic-organic coordinated complex of aluminum. The method comprises making an aqueous solution of aluminum chloride and aluminum bromide, mixing the solution with a polyhydroxy compound, heating the mixture and spray drying the mixture to obtain a product having a water content of about 1.0 to 10 weight percent. The inorganic-organic complexes are significantly soluble in non-aqueous medium.
U.S. Pat. No. 3,472,929 to Jones et al. teaches a method of making alcohol-soluble complexes of aluminum which consists of reacting a basic aluminum chloride and a polyhydroxy compound in an ethanol-water solution and distilling off the ethanol and water to a product which has 0.2 to 3.0 weight percent water. This invention produces alcohol soluble aluminum salts without the need for spray drying.
U.S. Pat. No. 3,507,896 to Jones et al., teaches a method of making alcohol soluble salts by reacting aluminum powder, a polyhydroxy compound and an acid in water, filtering the mixture and then drying the filtrate to remove water to form a product having from about 1.0 to 10 weight percent water.
U.S. Pat. No. 3,509,253 to Babbin, teaches an alcohol soluble complex of aluminum chloride. The complex is produced by reacting aluminum chloride or aluminum chlorhydroxide with an alcohol in an aqueous solution. The water is then removed by evaporation, crystallization or other means.
U.S. Pat. No. 3,523,130 to Jones et al., teaches a method of preparing inorganic-organic coordinated complex of aluminum comprising refluxing an aqueous solution of basic aluminum chloride and then reacting the refluxed aluminum chloride with a polyhydroxy compound and finally spray drying the reaction product to obtain a product having a water content of from 1.0 to 10 weight percent.
U.S. Pat. No. 3,523,153 to Holbert et al., teaches trichloro hydroxy aluminum derivatives in aerosol antiperspirant compositions. The trichloro hydroxy aluminum derivatives are produced by reacting aluminum chloride hexahydrate (dissolved in ethanol) with aluminum isoproplylate and recovering the reaction product produced.
U.S. Pat. No. 3,638,327 to Levy et al., teaches a method for making alcohol soluble aluminum chlorhydroxides by freeze drying the aluminum chlorhydroxide from an aqueous solution.
U.S. Pat. No. 3,876,758 to Beekman et al., teaches a method of making alcohol solutions of aluminum chlorhy-droxides for antiperspirant use. The process comprises reaction of a solution of aluminum chloride in an aliphatic alcohol with an aluminum chlorhydroxide-polyol composition. The aluminum chlorhydroxide polyol compositions are those taught in U.S. Pat. No. 3,359,169 to Slater et al.
U.S. Pat. No. 3,904,741 to Jones et al., teaches a method for the preparation of alcohol soluble basic aluminum chlorides. The method comprises controlling the molar ratio of aluminum to chloride and the amount of free and coordinated water in the solid. A preferred method is to heat an aluminum chloride solution having an Al:Cl ratio of about 1.9 under reflux for 2-4 hours and spray drying the solution to a friable solid having 18 to 20 weight percent of calculated free and coordinated water.
U.S. Pat. No. 3,947,556 to Jones et al., teaches a method for the preparation of alcohol soluble complexes of basic aluminum chlorides. The method comprises adding five-sixths basic aluminum chloride to a zinc halide or zirconyl bromide and drying the mixture to a substantially friable solid. The resulting solid contains about 12 to 30 weight percent water, are soluble in anhydrous alcohol and are compatible with halogenated hydrocarbons.
EP Patent Application No. 0007191 to Goslins et al. teaches a method of making aluminum chloride/polyhydroxide compound complexes by dissolving aluminum chlorhydrate and a polyhydroxide in water, heating the mixture and spray drying to a powder.
Most of the methods known in the art require the formation of the aluminum salt in an aqueous or aqueous/alcoholic medium, drying of the salt and then dissolving the salt in the alcoholic medium. These processes are inefficient because they require extreme control to ensure that the resulting salt is soluble in the alcoholic medium. Further, they have limited capability for producing alcoholic or other non-aqueous solutions of aluminum-zirconium halohydrates.
It is an object of the instant invention to show a method of producing non-aqueous solutions of aluminum and aluminum-zirconium compounds wherein the aluminum or aluminum-zirconium compound is formed "in-situ" in the non-aqueous solution.